#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003240.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003240 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 511 _journal_page_last 515 _publ_section_title ; A Solvate of the Diacetate Salt of the Octaethyltetraphenylporphyrin Dication, H~4~OETPP^2+^.2CH~3~COO^-^.3CH~3~COOH.CH~2~Cl~2~ ; _chemical_formula_sum 'C71 H84 Cl2 N4 O10' _chemical_formula_weight 1224.4 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 13.684(5) _cell_length_b 20.294(5) _cell_length_c 13.090(4) _cell_angle_alpha 98.64(2) _cell_angle_beta 107.98(3) _cell_angle_gamma 91.06(2) _cell_volume 3410.2 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_meas ? _diffrn_radiation_type 'CuK\a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 1.318 _cell_measurement_temperature 200 _exptl_crystal_description 'irregular block' _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour 'green' _chemical_compound_source 'from acetic acid/CH~2~Cl~2~ solution' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w-2\q' _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.6134 _exptl_absorpt_correction_T_max 0.7860 _diffrn_reflns_number 13038 _reflns_number_total 10077 _reflns_number_observed 6743 _reflns_observed_criterion F~o~>3\s(F~o~) _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 60 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'within counting statistics' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.095 _refine_ls_wR_factor_obs 0.119 _refine_ls_goodness_of_fit_obs 3.17 _refine_ls_number_reflns 6743 _refine_ls_number_parameters 784 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme '4F~o~^2^/[\s^2^(F~o~^2^)+(0.05F^2^)^2^]' _refine_ls_shift/esd_max 0.015 _refine_diff_density_max 0.90 _refine_diff_density_min -0.96 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source ? loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv N1 .6719(3) .7228(2) .4160(4) .029(1) N2 .5205(3) .7605(2) .2182(4) .024(1) N3 .6874(3) .7748(2) .1227(4) .024(1) N4 .8398(3) .7384(2) .3169(4) .026(1) C1 .7482(4) .6863(3) .4718(5) .028(2) C2 .7006(4) .6336(3) .5047(5) .031(2) C3 .5956(4) .6418(3) .4727(5) .034(2) C4 .5787(4) .6998(3) .4200(4) .030(2) C5 .4887(4) .7327(3) .3789(4) .025(2) C6 .4745(4) .7719(3) .2970(5) .027(2) C7 .4096(4) .8266(3) .2744(5) .027(2) C8 .4138(4) .8436(3) .1783(5) .027(2) C9 .4816(4) .7995(3) .1396(5) .025(2) C10 .5057(4) .7918(3) .0420(5) .025(2) C11 .5991(4) .7660(3) .0338(4) .025(2) C12 .6247(4) .7335(3) -.0584(5) .027(2) C13 .7299(4) .7275(3) -.0245(5) .028(2) C14 .7697(4) .7562(3) .0882(5) .026(2) C15 .8730(4) .7698(3) .1590(5) .025(2) C16 .8983(4) .7730(3) .2708(5) .025(2) C17 .9851(4) .8058(3) .3591(5) .027(2) C18 .9788(4) .7871(3) .4542(5) .027(2) C19 .8889(4) .7424(3) .4260(5) .025(2) C20 .8540(4) .7048(3) .4923(5) .029(2) C21 .7498(5) .5749(3) .5511(6) .045(2) C22 .7567(9) .5203(5) .4644(9) .109(5) C23 .5117(5) .5927(3) .4749(6) .047(2) C24 .4535(6) .5560(4) .3654(7) .072(3) C25 .3606(5) .8652(3) .3515(6) .044(2) C26 .4435(7) .9055(4) .4521(7) .082(4) C27 .3725(4) .9041(3) .1326(5) .039(2) C28 .4515(6) .9627(4) .1608(7) .073(3) C29 .5498(5) .7043(3) -.1680(5) .039(2) C30 .4892(7) .6430(4) -.1612(7) .085(4) C31 .7892(5) .6884(3) -.0895(5) .043(2) C32 .8098(8) .6222(4) -.0642(8) .094(5) C33 1.0620(4) .8585(3) .3540(5) .037(2) C34 1.0196(7) .9251(4) .3467(9) .091(4) C35 1.0433(4) .8171(3) .5665(5) .040(2) C36 .9898(7) .8692(4) .6217(6) .079(3) C37 .4039(4) .7253(3) .4261(5) .029(2) C38 .4198(5) .7396(4) .5380(5) .049(2) C39 .3416(5) .7322(4) .5810(6) .058(3) C40 .2429(5) .7111(4) .5109(6) .056(3) C41 .2246(4) .6964(4) .4012(6) .049(3) C42 .3022(4) .7041(3) .3569(5) .039(2) C43 .4331(4) .8129(3) -.0535(5) .030(2) C44 .3300(4) .7877(3) -.0924(5) .031(2) C45 .2611(5) .8112(3) -.1793(5) .041(2) C46 .2919(5) .8606(3) -.2254(5) .046(2) C47 .3933(5) .8853(3) -.1904(6) .049(2) C48 .4655(5) .8610(3) -.1049(5) .041(2) C49 .9526(4) .7844(3) .1085(5) .032(2) C50 .9368(5) .8317(3) .0385(5) .040(2) C51 1.0125(6) .8471(4) -.0038(6) .054(3) C52 1.1040(5) .8167(4) .0216(6) .051(3) C53 1.1192(4) .7682(4) .0869(6) .045(2) C54 1.0448(4) .7517(3) .1313(5) .039(2) C55 .9320(4) .6848(3) .5871(5) .030(2) C56 1.0139(5) .6478(3) .5702(5) .041(2) C57 1.0890(5) .6310(3) .6597(6) .048(3) C58 1.0861(5) .6501(4) .7640(6) .049(3) C59 1.0058(5) .6844(4) .7796(5) .052(3) C60 .9284(5) .7022(3) .6921(5) .039(2) O1 .7125(3) .8850(2) .2801(4) .046(1) O2 .7068(4) .8565(2) .4351(4) .049(2) C61 .7182(5) .8985(3) .3789(6) .035(2) C62 .7404(7) .9703(4) .4313(6) .064(3) O3 .5621(3) .6310(2) .1588(4) .046(1) O4 .7304(3) .6198(2) .2085(4) .045(1) C63 .6383(5) .5958(3) .1708(5) .040(2) C64 .6181(5) .5222(3) .1391(7) .065(3) O5 .7827(4) .9768(2) .2037(4) .064(2) O6 .7126(4) .9202(3) .0371(4) .075(2) C65 .7679(6) .9648(4) .0979(7) .048(3) C66 .8349(6) 1.0133(4) .0662(6) .062(3) O7 .3785(4) .5739(2) .1013(4) .062(2) O8 .3117(4) .6646(3) .0554(6) .107(3) C67 .3017(5) .6098(4) .0657(6) .045(3) C68 .1990(6) .5735(4) .0459(7) .074(3) O9 .8719(4) .5390(2) .2159(5) .081(2) O10 .9839(4) .6233(3) .2678(6) .105(3) C69 .9655(5) .5656(4) .2456(6) .052(3) C70 1.0458(6) .5162(5) .2482(10) .106(5) C1S .2965(8) .1081(6) .3353(11) .138(6) Cl1 .2027(4) .0452(2) .2477(3) .187(2) Cl2 .2931(3) .1753(3) .2645(5) .239(3) H21A .804300 .588200 .590900 ? H21B .717400 .558800 .590900 ? H22A .804300 .529400 .454500 ? H22B .695700 .500000 .431800 ? H22C .782600 .485300 .500000 ? H23A .543500 .558800 .522700 ? H23B .478300 .617600 .522700 ? H24A .500000 .529400 .340900 ? H24B .413000 .588200 .318200 ? H24C .391200 .529400 .363600 ? H25A .326100 .838200 .363600 ? H25B .326100 .897100 .318200 ? H26A .413000 .926500 .500000 ? H26B .478300 .867600 .477300 ? H26C .434800 .941200 .409100 ? H27A .347800 .897100 .068200 ? H27B .326100 .926500 .159100 ? H28A .478300 .970600 .227300 ? H28B .434800 1.00000 .113600 ? H28C .500000 .955900 .136400 ? H29A .587000 .691200 -.227300 ? H29B .500000 .735300 -.181800 ? H30A .456500 .617600 -.227300 ? H30B .543500 .617600 -.159100 ? H30C .478300 .632400 -.090900 ? H31A .760900 .691200 -.159100 ? H31B .847800 .705900 -.090900 ? H32A .856641 .627563 .015418 ? H32B .851709 .599779 -.103321 ? H32C .753474 .595855 -.068393 ? H33A 1.130400 .867600 .431800 ? H33B 1.065200 .852900 .295500 ? H34A .959348 .921594 .280155 ? H34B 1.067765 .956997 .340681 ? H34C .996012 .940210 .406131 ? H35A 1.043500 .794100 .613600 ? H35B 1.108700 .838200 .568200 ? H36A .969017 .902637 .582058 ? H36B 1.031210 .884785 .694154 ? H36C .926956 .845704 .627317 ? H38 .478300 .750000 .568200 ? H39 .347800 .735300 .659100 ? H40 .195700 .705900 .545500 ? H41 .152200 .691200 .363600 ? H42 .304300 .691200 .295500 ? H44 .304300 .750000 -.068200 ? H45 .195700 .794100 -.204500 ? H46 .260900 .882400 -.272700 ? H47 .413000 .911800 -.227300 ? H48 .543500 .882400 -.068200 ? H50 .869600 .852900 .022700 ? H51 1.000000 .882400 -.045500 ? H52 1.152200 .823500 .000000 ? H53 1.173900 .750000 .090900 ? H54 1.043500 .720600 .181800 ? H56 1.000000 .632400 .500000 ? H57 1.130400 .602900 .636400 ? H58 1.152200 .632400 .818200 ? H59 1.000000 .705900 .840900 ? H60 .869600 .720600 .704500 ? HN1 .682151 .758510 .379437 ? HN2 .543500 .720600 .204500 ? HN3 .695700 .808800 .181800 ? HN4 .782600 .705900 .272700 ? H62A .684839 .985526 .457828 ? H62B .746905 .997937 .380500 ? H62C .802089 .975807 .491335 ? H68A .195700 .544100 -.022700 ? H68B .152200 .602900 .045500 ? H68C .195700 .558800 .113600 ? H66A .879626 .988934 .034299 ? H66B .871019 1.045439 .124565 ? H66C .789388 1.035461 .009836 ? H64A .648178 .506463 .084475 ? H64B .546406 .510770 .113315 ? H64C .648504 .500979 .201568 ? H70A 1.084678 .526139 .201493 ? H70B 1.015004 .472597 .224055 ? H70C 1.092373 .519934 .320424 ? _cod_database_code 2003240